CN102699340A - Preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol - Google Patents

Preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol Download PDF

Info

Publication number
CN102699340A
CN102699340A CN2012101073354A CN201210107335A CN102699340A CN 102699340 A CN102699340 A CN 102699340A CN 2012101073354 A CN2012101073354 A CN 2012101073354A CN 201210107335 A CN201210107335 A CN 201210107335A CN 102699340 A CN102699340 A CN 102699340A
Authority
CN
China
Prior art keywords
active oxygen
nano silver
white transparency
water white
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2012101073354A
Other languages
Chinese (zh)
Other versions
CN102699340B (en
Inventor
不公告发明人
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANGHAI SHANGXING HOUSEHOLD GOODS CO Ltd
Original Assignee
SHANGHAI SHANGXING HOUSEHOLD GOODS CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SHANGHAI SHANGXING HOUSEHOLD GOODS CO Ltd filed Critical SHANGHAI SHANGXING HOUSEHOLD GOODS CO Ltd
Priority to CN201210107335.4A priority Critical patent/CN102699340B/en
Publication of CN102699340A publication Critical patent/CN102699340A/en
Application granted granted Critical
Publication of CN102699340B publication Critical patent/CN102699340B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)

Abstract

The invention relates to a preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol. Firstly a silver-bearing oxidizing agent and a protective agent are soluble in water to prepare oxidation solution, a reducing agent is soluble in water to form reducing solution, the oxidation solution is added in the reducing solution to form mixed liquor; then reactive oxygen solution is slowly dropped in the oxidation solution under the condition of 50-100rpm of the stirring speed, the PH value is adjusted to be 6-7 by using 0.25% ammonia solution after dropping is completed, the solution is sufficiently stirred and mixed for 10-30min, and the solution is placed in a reaction still with a backflow device for reaction for 1-4 hours under the condition of 50-500rpm of the stirring speed at 100-160 DEG C to obtain the colourless transparent nanometer silver solution; finally reactive oxygen is added in the nanometer silver sol to prepare the colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol according to proportion. The preparation method has high-efficient, rapid and everlasting sterilization performance, high stability and good dispersibility, can be directly used in fields such as spinning, medical treatment, environmental protection and household appliances.

Description

A kind of preparation method of water white transparency quick sterilization active oxygen composite Nano silver sol
Technical field
The present invention relates to a kind of Nano Silver preparation methods, particularly a kind of preparation method of water white transparency quick sterilization active oxygen composite Nano silver sol.
Background technology
Recently, along with the raising day by day of living standard, people have had higher requirement to peripheral living environment.For example, people pay attention to its durable antibiotic performance for the various commodity of aspects such as relating to clothing, food, live, go very much.And the inorganic antiseptic that is usually used at present on the commodity is mainly the powder antiseptic; Like the inorganic antiseptic of metal ions such as mercurous, plumbous, nickel, copper, zinc, gold, but the general decentralization of these antiseptics intersects, and metal ion such as its mercury that comprises, lead, copper, zinc, gold or human body had the murder by poisoning of residual; Or object there is coloration; Or bactericidal property a little less than, or cost is too high, and is difficult to apply.
Nano silver colloidal sol receives people's favor as a kind of inorganic, wide spectrum, long-acting, antiseptic that have no side effect, thereby application constantly enlarges.Compare with common silver, therefore Nano Silver uses the Nano Silver of minute quantity just can produce very strong antibacterial effect because the silver particles that its unit volume of specific area ambassador discharges is more.Research shows that Nano Silver all has good antibacterial ability to more than 650 kind of bacterium such as Gram-positive and negative bacteria, fungi and bacillus, therefore can be applied to fields such as weaving, health care, environmental protection and daily electrical home appliance widely.But, thereby make the too high or low concentration bactericidal property of use financial cost of existing nano silver colloidal sol bad and its scope of application is dwindled greatly because the sterilization mechanism of nano silver colloidal sol needs the kill microorganisms that high concentration for a long time could be good for the contact sterilization.Existing in addition nano silver colloidal sol is generally black liquor or is that yellow colloid perhaps is low concentration water white transparency colloid, causes look change problem in the meeting usually if directly apply it to textile and commodity.Therefore, the preparation method of preparation water white transparency quick sterilization active oxygen composite Nano silver sol has urgent application demand and huge economic.This water white transparency quick sterilization active oxygen composite Nano silver sol has remedied the independent Nano Silver bad shortcoming of bactericidal effect at short notice.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of water white transparency quick sterilization active oxygen composite Nano silver sol; Have the active oxygen composite Nano silver sol of good quick sterilization and high-efficient and lasting anti-microbial property with preparation, thereby overcome the deficiency that Nano Silver in the prior art can not quick sterilization.
For realizing the foregoing invention purpose, the present invention has adopted following technical scheme:
A kind of preparation method of water white transparency quick sterilization active oxygen composite Nano silver sol.It is characterized in that said method is:
At first with argentiferous oxidant and the protective agent oxidizing solution of processing soluble in water, and in addition with reducing agent formation reducing solution soluble in water, oxidizing solution and reducing solution are mixed the formation mixed solution.Secondly, with active oxygen be added drop-wise in the mixed liquor with 0.25% ammoniacal liquor regulate pH value behind 6-7 fully stirring 10-30min make reactant liquor.
Thereafter, it is 110~160 ℃ that its reactant liquor is placed on temperature, and reaction obtained the water white transparency nano silver colloidal sol in 1-4 hour in the back flow reaction still of mixing speed under the condition of 50~500rpm
At last, active oxygen is proportionally added to make water white transparency quick sterilization composite Nano silver sol in the water white transparency nano silver colloidal sol.This colloidal sol degree is the water white transparency colloid when being 0~2000mg/kg, when content of nanometer silver is 0.2% for the 100mg/kg active o content and the sterilizing rate of Gram-negative bacteria Escherichia coli and gram-positive bacteria staphylococcus aureus effect 5min can both reach 99.9%.
Concretely, this method specifically comprises the following step:
A. with argentiferous oxidant, protective agent and water by 0.01~0.5: 0.01~5: 1000 mass ratio is mixed with oxidizing solution; With reducing agent and water with 0.1~10: 10~1000 mol ratio is mixed with reducing solution; Oxidizing solution and reducing solution are mixed the formation mixed solution.
B. active oxygen is added drop-wise in the mixed liquor and regulates pH value with 0.25% ammoniacal liquor and behind 6-7, fully stir 10-30min and make reactant liquor.The mol ratio that makes active oxygen and oxidant is 0.001~0.1: 0.0005~0.01.
C. reactant liquor being placed on temperature is 110~160 ℃, and reaction obtained the water white transparency nano silver colloidal sol in 1-4 hour in the back flow reaction still of mixing speed under the condition of 50~500rpm
D. active oxygen is proportionally added in the water white transparency nano silver colloidal sol and stir 10-30min and make water white transparency quick sterilization composite nano silver.
In step b, the time that mixes reaction solution is 1min~1h.
Preferable methods is:
Silver nitrate and protective agent and water is water-soluble with 1: 1: 500~1000 mass ratio, be prepared into oxidizing solution; With reducing agent and water with 1~50: 100 mol ratio is mixed with reducing solution; Oxidizing solution and reducing solution are mixed the formation mixed solution.
Active oxygen added in the mixed solution with 0.25% ammoniacal liquor regulate pH value to about the 6-7, forming reactant liquor, to make the mol ratio of active oxygen and oxidant be 10~50: 1.
It is that 140 ℃, mixing speed are that the reaction kettle for reaction that 250rpm has a backflow made water white transparency nano silver colloidal sol liquid in 4 hours that reaction solution is placed into heating-up temperature, and wherein the average grain diameter of nano silver particles is at 20~30nm.
Active oxygen is added drop-wise to the water white transparency nano silver colloidal sol stirs 20min, making active oxygen and mol ratio Nano Silver is 0.005: 0.0005~0.001.
Said argentiferous oxidant is silver nitrate or silver thiosulfate.
Said reducing agent is ethylene glycol or glycerine or propane diols.
Said protective agent is one or several the combination in amino acid, polyvinyl alcohol, detergent alkylate sodium sulfonate and the polyvinylpyrrolidone.
Described active oxygen is a food-grade active oxygen or for the AG active oxygen or for the technical grade active oxygen.
The present invention passes through argentiferous oxidant (like silver nitrate) and weak reductant (alcohols) to be 110-160 ℃ in temperature after its pH value is controlled at 6-7 through using weak aqua ammonia to regulate after adding active oxygen (both can be that reducing agent also is a stabilizing agent); Mixing speed is to react after 1-4 hour under the condition of 50~500r pm to make nano silver colloidal sol; Again active oxygen is dripped according to certain ratio and make water white transparency quick sterilization active oxygen composite Nano silver sol after nano silver colloidal sol stirs certain hour; And the nano silver particles particle diameter of preparation is controlled; High stability is dispersed with better, and has quick, high-efficient and lasting bactericidal property.Silver content is 0.1% o'clock and Escherichia coli for the 100mg/kg active o content, and its sterilizing rate can both reach 99.9% behind staphylococcus aureus and the Candida albicans effect 5min.Make Nano Silver see that light can not become by look as if this composite Nano silver sol being sprayed directly on oxidation certain of cloth and body surface and discoloration, and the antibacterial activity value of antibiotic cloth can reach 3 owing to hydrogen peroxide has.The surface that this water white transparency quick sterilization active oxygen composite Nano silver sol directly is sprayed onto articles for daily use has fast, the bactericidal property of high-efficient and lasting.
Compared with prior art; Beneficial effect of the present invention is: preparation method's technology of this water white transparency quick sterilization composite Nano silver sol is simple, big easily production, and preparation advantages of nontoxic raw materials evil; And the composite Nano silver colloid that makes has fast, the high-efficient and lasting bactericidal property; High stability is dispersed with better, and is sprayed onto body surface and sees that light look can not take place becomes, and can be widely used in being applied to fields such as weaving, health care, environmental protection and daily electrical home appliance.
The specific embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is done further explain.
The preparation method of embodiment 1 this water white transparency quick sterilization active oxygen composite Nano silver sol may further comprise the steps:
2.5g polyvinyl alcohol and 0.95g silver nitrate solid joined in the 3.0L deionized water dissolve, be prepared into oxidizing solution; 50g ethylene glycol joined in the 1.8L water dissolve, be mixed with reducing solution; Oxidizing solution and reducing solution are mixed with mixed solution.
The 5g active oxygen is added drop-wise in the mixed solution to use 0.25% ammoniacal liquor to regulate pH value be 6 to make reaction solution;
It is that the reaction kettle for reaction that 250rpm has a reflux made the water white transparency nano silver colloidal sol in 1 hour that reaction solution is placed into 140 ℃ of mixing speeds.
Food-grade active oxygen (30%) 20g added in the water white transparency nano silver colloidal sol stir 30min and make water white transparency quick sterilization active oxygen composite Nano silver sol, obtain the Nano Silver average grain diameter at 20nm.
At first, measure according to Fo Erhadefa, silver content is 100mg/kg in this nano silver colloid;
According to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard, test the bactericidal property of this water white transparency quick sterilization active oxygen composite Nano silver sol, test result and result such as following table thereafter:
Test result
Figure BSA00000700372200061
Test result
Test result shows that this water white transparency quick sterilization active oxygen composite Nano silver sol has good stability and lasting bactericidal property;
At last its water white transparency quick sterilization active oxygen composite Nano silver sol is sprayed directly on the white cotton and cotton is placed into the sun directly shines and look local did not take place in 10 days become.According to its antibacterial effect of JIS L1902-2008 test, test result shows that the antibacterial activity value of this antibiotic cloth reaches 3 with its cotton.Anti-bacteria test result is following:
Figure BSA00000700372200062
Can know that by this test result this water white transparency quick sterilization active oxygen composite Nano silver sol has good bactericidal property.It is to Gram-negative bacteria staphylococcus aureus and gram-positive bacteria Escherichia coli and can both reach more than 99% to the sterilizing rate of the representative bacterium Candida albicans effect 5min of fungi; Under same concentration, generally have only about 50% and contain independent Nano Silver with the sterilizing rate of bacterial action 5min;
Then; This water white transparency quick sterilization active oxygen composite Nano silver sol is placed in 54 ℃ of insulating boxs placed 14 days; Taking out the back finds; It still is a water white transparency colloidal sol, and simultaneously according to QB/T2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard, test result and result are following:
Test result
Figure BSA00000700372200071
Test result
Test result shows that this water white transparency quick sterilization active oxygen composite Nano silver sol has good stability and lasting bactericidal property;
At last its water white transparency quick sterilization active oxygen composite Nano silver sol is sprayed directly on the white cotton and cotton is placed into the sun directly shines and look local did not take place in 10 days become.According to its antibacterial effect of JIS L1902-2008 test, test result shows that the antibacterial activity value of this antibiotic cloth reaches 3 with its cotton.Anti-bacteria test result is following:
Figure BSA00000700372200082
The preparation method of embodiment 2 these nano silver colloidal sol for preventing color change may further comprise the steps:
50g amino acid and 47.5g silver nitrate solid joined in the 1L deionized water dissolve, be prepared into oxidizing solution, the 2L glycerine is joined in the 18L water dissolve, be mixed with reducing solution, with oxidizing solution and reducing solution mixed mixed solution.
1L is analyzed pure active oxygen (30%) to be added drop-wise in the mixed liquor back and to make reaction solution with 0.25% ammoniacal liquor adjusting pH value to 7.
Reaction solution is placed into 120 ℃ of temperature, and mixing speed is that the reaction kettle for reaction that has reflux of 350r pm makes the water white transparency nano silver colloidal sol after 4 hours.Measure according to Fo Erhadefa, the silver content 1000mg/kg of this nano silver colloid simultaneously, is dried the back with this colloidal sol and is determined that it is silver-colored simple substance with XRD analysis in 80 ℃ of baking ovens.
Thereafter, with after 10 times of this water white transparency nano silver colloid dilutions with active oxygen in proportion (making the mol ratio of active oxygen and simple substance silver is 30: 1) add to wherein the back fully stirring made water white transparency quick sterilization active oxygen composite Nano silver sol in 1 hour.According to its sterilizing rate with Escherichia coli, staphylococcus aureus and Candida albicans effect 5min of QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test all is 99%.
Then; With this water white transparency quick sterilization active oxygen composite Nano silver sol be placed in 54 ℃ of insulating boxs place 14 days after; Find that its proterties is constant, and according to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test itself and Escherichia coli.The sterilizing rate of staphylococcus aureus and Candida albicans effect 5min all is 99%.
At last; Water white transparency quick sterilization active oxygen composite Nano silver sol is sprayed at makes antibiotic cloth on the cotton, this cloth adopts its antibacterial effect of JIS L1902-2008 test, and the result shows; The antibacterial activity value of this antibiotic cloth reaches 3, and the look change does not take place cloth.
The preparation method of embodiment 3 water white transparency quick sterilization active oxygen composite Nano silver sols may further comprise the steps:
15g polyvinylpyrrolidone, 10g benzene sulfonic acid sodium salt and 25g silver nitrate are dissolved in the 2L deionized water; Be mixed with oxidizing solution; The 2Kg glycerine to going in the 2.7L deionized water dissolving preparation reducing solution, is made mixed solution with after oxidizing solution and the reducing solution mixing.
Be added drop-wise in the mixed liquor 1L food-grade active oxygen (30%) back with making reaction solution about 0.25% ammoniacal liquor adjusting pH value to 6.5;
Reaction solution is placed into 160 ℃ of temperature, and mixing speed is that the reaction kettle for reaction that has reflux of 150rpm makes the water white transparency nano silver colloidal sol after 3 hours.Measure according to Fo Erhadefa, the silver content 2000mg/kg of this nano silver colloid simultaneously, is dried the back with this colloidal sol and is determined that it is silver-colored simple substance with XRD analysis in 80 ℃ of baking ovens.
Thereafter, with after 20 times of this water white transparency nano silver colloid dilutions with active oxygen in proportion (making the mol ratio of active oxygen and simple substance silver is 30: 1) add to wherein the back fully stirring 45min make the water white transparency quick sterilization and make water white transparency quick sterilization active oxygen composite Nano silver sol.According to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test itself and Escherichia coli.The sterilizing rate of staphylococcus aureus and Candida albicans effect 5mi n all is 99%.
Then; With this water white transparency quick sterilization active oxygen composite Nano silver sol be placed in 54 ℃ of insulating boxs place 14 days after; Find that its proterties is constant, and according to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test itself and Escherichia coli.The sterilizing rate of staphylococcus aureus and Candida albicans effect 5min all is 99%.
At last; Water white transparency quick sterilization active oxygen composite Nano silver sol is sprayed at makes antibiotic cloth on the cotton, this cloth adopts its antibacterial effect of JIS L1902-2008 test, and the result shows; The antibacterial activity value of this antibiotic cloth reaches 3, and the look change does not take place cloth.
The preparation method that embodiment 4 water white transparency quick sterilization active oxygen composite Nano silver sols are somebody's turn to do may further comprise the steps:
100g polyvinylpyrrolidone, 50g benzene sulfonic acid sodium salt and 20.6g silver thiosulfate are dissolved in the 3L deionized water, are mixed with oxidizing solution; Dissolving preparation reducing solution mixes the formation mixed solution with oxidizing solution and reducing solution in the 3.5L deionized water to going into the 0.5kg glycerine.
Be added drop-wise in the mixed liquor 0.5L food-grade active oxygen (30%) back with making reaction solution about 0.25% ammoniacal liquor adjusting pH value to 6.5.
Reaction solution is placed into 110 ℃ of temperature, and mixing speed is that the reaction kettle for reaction that has reflux of 500rpm makes the water white transparency nano silver colloidal sol after 4 hours.Measure according to Fo Erhadefa, the silver content 1500mg/kg of this nano silver colloid simultaneously, is dried the back with this colloidal sol and is determined that it is silver-colored simple substance with XRD analysis in 80 ℃ of baking ovens.
Thereafter, with after 20 times of this water white transparency nano silver colloid dilutions with active oxygen in proportion (making the mol ratio of active oxygen and simple substance silver is 60: 1) add to wherein the back fully stirring 45min make water white transparency quick sterilization active oxygen composite Nano silver sol.According to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test itself and Escherichia coli.The sterilizing rate of staphylococcus aureus and Candida albicans effect 5min all is 99%.
Then; With this water white transparency quick sterilization active oxygen composite Nano silver sol be placed in 54 ℃ of insulating boxs place 14 days after; Find that its proterties is constant, and according to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test itself and Escherichia coli.The sterilizing rate of staphylococcus aureus and Candida albicans effect 5min all is 99%.
At last; Water white transparency quick sterilization active oxygen composite Nano silver sol is sprayed at makes antibiotic cloth on the cotton, this cloth adopts its antibacterial effect of JIS L1902-2008 test, and the result shows; The antibacterial activity value of this antibiotic cloth reaches 3, and the look change does not take place cloth.
The preparation method of embodiment 5 water white transparency quick sterilization active oxygen composite Nano silver sols may further comprise the steps:
0.5g polyvinylpyrrolidone, 0.5g benzene sulfonic acid sodium salt and 0.1g silver nitrate are dissolved in the 1L deionized water, are mixed with oxidizing solution, with the 20g propane diols to going in the 180ml deionized water dissolving preparation reducing solution; With making mixed solution after oxidizing solution and the reducing solution mixing.
Be added drop-wise in the mixed liquor 0.05L technical grade active oxygen (30%) back with making reaction solution about 0.25% ammoniacal liquor adjusting pH value to 6.5.
Reaction solution is placed into 120 ℃ of temperature, and mixing speed is that the reaction kettle for reaction that has reflux of 50rpm makes the water white transparency nano silver colloidal sol after 4 hours.Measure according to Fo Erhadefa, the silver content 50mg/kg of this nano silver colloid simultaneously, is dried the back with this colloidal sol and is determined that it is silver-colored simple substance with XRD analysis in 80 ℃ of baking ovens.
Thereafter, adding to the 0.5L active oxygen wherein, the abundant 45min of stirring in back makes water white transparency quick sterilization active oxygen composite Nano silver sol.According to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test itself and Escherichia coli.The sterilizing rate of staphylococcus aureus and Candida albicans effect 5min all is 99%.
Then; With this water white transparency quick sterilization active oxygen composite Nano silver sol be placed in 54 ℃ of insulating boxs place 14 days after; Find that its proterties is constant, and according to QB/T 2738-2005 daily chemical products antibacterial bacteriostatic Evaluation on effect method standard test itself and Escherichia coli.The sterilizing rate of staphylococcus aureus and Candida albicans effect 5min all is 99%.
At last; Water white transparency quick sterilization active oxygen composite Nano silver sol is sprayed at makes antibiotic cloth on the cotton, this cloth adopts its antibacterial effect of JIS L1902-2008 test, and the result shows; The antibacterial activity value of this antibiotic cloth reaches 2, and the look change does not take place cloth.
The foregoing description is merely explanation technical conceive of the present invention and characteristics, and its purpose is to let the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.

Claims (10)

1. the preparation method of a water white transparency quick sterilization active oxygen composite Nano silver sol is characterized in that said method is:
At first, argentiferous oxidant and protective agent is soluble in water, make oxidizing solution, and in addition direct behind the reducing agent formation reducing solution soluble in water and oxidizing solution mixing are obtained mixed solution; Secondly, with active oxygen be added drop-wise in the mixed liquor with 0.25% ammoniacal liquor regulate pH value behind 6-7 fully stirring 10-30min make reactant liquor.
Thereafter, it is 110~160 ℃ that its reactant liquor is placed on temperature, and reaction obtained the water white transparency nano silver colloidal sol in 1-4 hour in the back flow reaction still of mixing speed under the condition of 50~500rpm.
At last, active oxygen is proportionally added to make water white transparency quick sterilization active oxygen composite Nano silver sol in the water white transparency nano silver colloidal sol.This colloidal sol degree is the water white transparency colloid when being 0~1000mg/kg, when content of nanometer silver is 1.0% for the 50mg/kg active o content and the sterilizing rate of Gram-negative bacteria Escherichia coli and gram-positive bacteria staphylococcus aureus effect 5min can both reach 99.9%.
2. the preparation method of water white transparency quick sterilization active oxygen composite Nano silver sol according to claim 1 is characterized in that this method specifically comprises the following step:
A. with argentiferous oxidant, protective agent and water by 0.1~60: 1~50: 1000 mass ratio is mixed with oxidizing solution; With reducing agent and water with 1~50: 10~1000 mol ratio is mixed with reducing solution; Oxidizing solution and reducing solution mixing are obtained mixed solution.Wherein, the mol ratio of argentiferous oxidant and reducing agent is 1: 10~20.
B. active oxygen is added drop-wise to and uses weak aqua ammonia to regulate pH value in the mixed liquor fully to stir 10-30min after as 6-7, make reactant liquor.
C. reactant liquor is placed into 110-160 ℃, mixing speed has reaction kettle for reaction 1-4 hour of reflux and obtains the water white transparency nano silver colloidal sol under the condition of 50~500rpm.
D. active oxygen is proportionally added to and make water white transparency quick sterilization composite Nano silver sol in the water white transparency nano silver colloidal sol.
3. the preparation method of water white transparency quick sterilization nano silver colloidal sol according to claim 2 is characterized in that, in step b, the ratio of adding active oxygen is that the mol ratio of active oxygen and oxidant is 2~200: 1.
4. the preparation method of water white transparency quick sterilization nano silver colloidal sol according to claim 2.Its characteristic, in step c, reaction temperature 110-160 ℃, in the back flow reaction still under the condition of mixing speed 50~500rpm reaction time 1-4 hour.
5. the preparation method of water white transparency quick sterilization nano silver colloidal sol according to claim 2, its characteristic, in steps d, the ratio of adding active oxygen is the molar ratio 10~100: 1 of active oxygen and Nano Silver.
6. the preparation method of water white transparency quick sterilization active oxygen composite Nano silver sol according to claim 1 and 2 is characterized in that this method is:
Silver nitrate and protective agent is water-soluble, be prepared into oxidizing solution; With the water-soluble reducing solution of processing of reducing agent, with oxidizing solution and the mixed mixed solution that gets of reducing solution.
Active oxygen is added drop-wise to uses after the mixed liquor weak aqua ammonia to regulate pH value fully to stir 10-30min after as 6-7, make reactant liquor.
Reactant liquor is placed on 110-160 ℃, and mixing speed has reaction kettle for reaction 1-4 hour of reflux and obtains the water white transparency nano silver colloidal sol under the condition of 50~500rpm, and wherein the average grain diameter of nano silver particles is at 7~300nm.
7. the preparation method of water white transparency quick sterilization active oxygen composite Nano silver sol according to claim 1 and 2 is characterized in that said argentiferous oxidant is silver nitrate or silver thiosulfate.
8. according to the preparation method of claim 1 or 2 or 6 described water white transparency quick sterilization active oxygen composite Nano silver sols, said reducing agent is ethylene glycol or glycerine or propane diols.
9. be food-grade active oxygen or for the AG active oxygen or be the technical grade active oxygen according to the said active oxygen of preparation method of claim 1 or 2 or 6 described water white transparency quick sterilization active oxygen composite Nano silver sols.
10. according to the preparation method of claim 1 or 2 or 6 described water white transparency quick sterilization active oxygen composite Nano silver sols, said protective agent is one or several the combination in amino acid, polyvinyl alcohol, dodecyl sodium sulfonate and the polyvinylpyrrolidone.
CN201210107335.4A 2012-04-13 2012-04-13 Preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol Expired - Fee Related CN102699340B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210107335.4A CN102699340B (en) 2012-04-13 2012-04-13 Preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210107335.4A CN102699340B (en) 2012-04-13 2012-04-13 Preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol

Publications (2)

Publication Number Publication Date
CN102699340A true CN102699340A (en) 2012-10-03
CN102699340B CN102699340B (en) 2015-04-01

Family

ID=46892556

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210107335.4A Expired - Fee Related CN102699340B (en) 2012-04-13 2012-04-13 Preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol

Country Status (1)

Country Link
CN (1) CN102699340B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1128188A (en) * 1995-09-29 1996-08-07 中国科学院固体物理研究所 Size-controllable preparation method of nanometer-level silver
CN1729787A (en) * 2005-08-08 2006-02-08 深圳清华大学研究院 Liquid nanometer simple substance silver antibacterial agent and preparation method thereof
KR100750196B1 (en) * 2006-06-12 2007-08-17 주식회사 국일인토트 Manufacturing method of leather nano silver anti bacteria and leather goods
CN101168070A (en) * 2007-10-09 2008-04-30 洛阳民康生物工程有限公司 Air sterilization cleaning agent
CN101473845A (en) * 2009-01-19 2009-07-08 上海华实纳米材料有限公司 Method for preparing nano silver colloidal sol for preventing color change
CN101633045A (en) * 2009-08-24 2010-01-27 北京崇高纳米科技有限公司 Nanometer silver collosol, preparation method and application thereof
CN102190953A (en) * 2010-03-12 2011-09-21 周刚 Production method of solvent-type antibacterial paint

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1128188A (en) * 1995-09-29 1996-08-07 中国科学院固体物理研究所 Size-controllable preparation method of nanometer-level silver
CN1729787A (en) * 2005-08-08 2006-02-08 深圳清华大学研究院 Liquid nanometer simple substance silver antibacterial agent and preparation method thereof
KR100750196B1 (en) * 2006-06-12 2007-08-17 주식회사 국일인토트 Manufacturing method of leather nano silver anti bacteria and leather goods
CN101168070A (en) * 2007-10-09 2008-04-30 洛阳民康生物工程有限公司 Air sterilization cleaning agent
CN101473845A (en) * 2009-01-19 2009-07-08 上海华实纳米材料有限公司 Method for preparing nano silver colloidal sol for preventing color change
CN101633045A (en) * 2009-08-24 2010-01-27 北京崇高纳米科技有限公司 Nanometer silver collosol, preparation method and application thereof
CN102190953A (en) * 2010-03-12 2011-09-21 周刚 Production method of solvent-type antibacterial paint

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
宋建恒等: "双氧水还原制备超细银粉", 《中国有色金属学报》 *
陆伟杰: "制备纳米银粉技术的研究", 《湖州师范学院学报》 *

Also Published As

Publication number Publication date
CN102699340B (en) 2015-04-01

Similar Documents

Publication Publication Date Title
CN101473845B (en) Method for preparing nano silver colloidal sol for preventing color change
CN104145993B (en) A kind of chitosan and silver-bearing copper are blended the method preparing complex antimicrobials
CN101999412B (en) Nano-silver solution and preparation method thereof
CN101044848B (en) Nanometer silver antibiotic powder fixed by silk fibroin and preparation method thereof
CN103783079A (en) Preparation method of silver-loaded mesoporous inorganic antibacterial agent
CN101926363B (en) Method for preparing liquid antibacterial agent containing complex silver
CN1298222C (en) Liquid nanometer simple substance silver antibacterial agent and preparation method thereof
CN101669520A (en) Air conditioning filter screen bacteriostatic agent and preparation method thereof as well as preparation method of air conditioning filter screen
CN104824020A (en) Preparation method of nanometer titanium dioxide composite nanometer silver sol
CN105296192A (en) Nano silver added powerful sterilizing and lasting bacteria-resisting laundry detergent and manufacturing method therefor
CN101347127A (en) Novel surrounding purifying material as well as preparation and use thereof
CN101015300A (en) Silver-containing antibacterial agent
CN105648745B (en) Fabric polymer matrix cerium-doped nanometer zinc oxide composite antibiosis agent and preparation method thereof
CN103127933A (en) Nano cerium oxide silver-loaded catalyst, manufacturing method and purpose thereof
CN1623897A (en) Process for preparing silicon dioxide of carrying nano silver
CN110184137B (en) Silver ion antibacterial microemulsion, preparation method thereof and application thereof in laundry detergent
CN106860033A (en) Washing-free antibacterial is washed one's hands gel and preparation method thereof
CN102699340B (en) Preparation method of colourless transparent rapid sterilization reactive oxygen composite nanometer silver sol
CN103981698B (en) A kind of nano-silver antibacterial finishing agent and preparation method thereof
CN111876273A (en) Sterilization laundry detergent based on hydrophilic zinc oxide, preparation method and application thereof
CN112144277A (en) Fabric antibacterial treatment fluid and preparation method thereof
CN106880507A (en) Washing-free antibacterial hand sanitizer and preparation method thereof
JP2002068915A (en) Sol
CN102578148A (en) Method for improving antibacterial property of tetrapod-like zinc oxide whisker
CN1623898A (en) Process for preparing silicon gel carrying silver ion

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
DD01 Delivery of document by public notice
DD01 Delivery of document by public notice

Addressee: Patent of Shanghai Shangxing Household Products Co., Ltd. The person in charge

Document name: Payment Notice

CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20150401